WO2009144036A1 - Electroplating additive for the deposition of metal, a binary, ternary, quaternary or pentanary alloy of elements of group 11 (ib)-group 13 (iiia) -group 16 (via) - Google Patents

Electroplating additive for the deposition of metal, a binary, ternary, quaternary or pentanary alloy of elements of group 11 (ib)-group 13 (iiia) -group 16 (via) Download PDF

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Publication number
WO2009144036A1
WO2009144036A1 PCT/EP2009/003885 EP2009003885W WO2009144036A1 WO 2009144036 A1 WO2009144036 A1 WO 2009144036A1 EP 2009003885 W EP2009003885 W EP 2009003885W WO 2009144036 A1 WO2009144036 A1 WO 2009144036A1
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WO
WIPO (PCT)
Prior art keywords
group
copper
plating
indium
metal
Prior art date
Application number
PCT/EP2009/003885
Other languages
English (en)
French (fr)
Inventor
Torsten Voss
Jörg SCHULZE
Andreas Kirbs
Aylin Sönmez
Heiko Brunner
Bernd Fröse
Ulrike Engelhardt
Original Assignee
Atotech Deutschland Gmbh
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Atotech Deutschland Gmbh filed Critical Atotech Deutschland Gmbh
Priority to US12/995,078 priority Critical patent/US8828278B2/en
Priority to JP2011510899A priority patent/JP5286410B2/ja
Priority to CN2009801194459A priority patent/CN102047438B/zh
Publication of WO2009144036A1 publication Critical patent/WO2009144036A1/en

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Classifications

    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L31/0248—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies
    • H01L31/0256—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by the material
    • H01L31/0264—Inorganic materials
    • H01L31/032—Inorganic materials including, apart from doping materials or other impurities, only compounds not provided for in groups H01L31/0272 - H01L31/0312
    • H01L31/0322—Inorganic materials including, apart from doping materials or other impurities, only compounds not provided for in groups H01L31/0272 - H01L31/0312 comprising only AIBIIICVI chalcopyrite compounds, e.g. Cu In Se2, Cu Ga Se2, Cu In Ga Se2
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C335/00—Thioureas, i.e. compounds containing any of the groups, the nitrogen atoms not being part of nitro or nitroso groups
    • C07C335/04—Derivatives of thiourea
    • C07C335/16—Derivatives of thiourea having nitrogen atoms of thiourea groups bound to carbon atoms of six-membered aromatic rings of a carbon skeleton
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/38—Electroplating: Baths therefor from solutions of copper
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/56—Electroplating: Baths therefor from solutions of alloys
    • C25D3/58—Electroplating: Baths therefor from solutions of alloys containing more than 50% by weight of copper
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L31/04—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof adapted as photovoltaic [PV] conversion devices
    • H01L31/06—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof adapted as photovoltaic [PV] conversion devices characterised by potential barriers
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00—Energy generation through renewable energy sources
    • Y02E10/50—Photovoltaic [PV] energy
    • Y02E10/541—CuInSe2 material PV cells

Definitions

  • the present invention relates to electroplating additives for the deposition of a group IB metal/binary or ternary group IB-group IMA/ternary, quaternary or pen-y group IB-group IIIA-group VIA alloy on substrates useful for thin film solar cells. Further, the invention relates to a process for the preparation of these additives and their use in a metal plating composition.
  • US patent 7,026,258 B2 concerns a method for making thin-film CIGS which consists in: electrochemically depositing on a substrate a layer of stoichiometry close to CuInSe 2 ; then rapidly annealing said layer from a light source with pulses of sufficient power to recrystallise CIS.
  • the electrodeposited elements are premixed.
  • a homogeneous matrix is obtained which can support sudden temperature increases during the rapid annealing.
  • the total layer thickness of the alloy deposition varies with a standard deviation of more than 8 %. The inhomogeneities caused by hydrodynamics, potential and current density drops are clearly visible. Deposition was performed on a 15 x 15 cm 2 molybdenum float glass material (centered plotted measurement area 10 x 10 cm 2 ).
  • Fig. 3 shows an XRF surface scan and plot of the total layer thickness obtained in Example 1 according the present invention.
  • Figs. 7a and 7b show the stoichiometry (Cu/ln ratio) of electrodeposited CISe precursor in relation to a) the applied potential and b) the applied current density on Mo coated float glass as well as the electrolyte behaviour according to invention (Example 1 ).
  • the horizontal sections of both curves show the ranges wherein a homogeneous alloy composition can be obtained using the additives according to the present invention.
  • An and Ar 2 represent a phenylene or naphthylene radical.
  • the groups FGi and FG2 are substituents for the An, Ar 2 , Heti and Het 2 radicals and are selected from the group consisting of -S(O) 2 OH, -S(O)OH, -COOH, -P(O) 2 OH and primary, secondary and tertiary amino groups and salts and esters thereof.
  • Suitable esters are alkyl esters and, in particular, C 1 - 6 alkyl esters wherein C 1 - 6 alkyl means straight and branched chain saturated hydrocarbon monovalent radicals having from 1 to 6 carbon atoms such as, for example, methyl, ethyl, propyl, n-butyl, 1 -methylethyl, 2-methylpropyl, 1 ,1 -dimethylethyl, 2-methylbutyl, n-pentyl, dimethylpropyl, n-hexyl, 2-methylpentyl, 3-methylpentyl, and the like.
  • n 1 is 2 to 12, preferably 2 to 8.
  • X 1 , X 2 , FGi, FG 2 , m and n are as defined herein before with a diamine compound of the formula H 2 N-R-NH 2 , wherein R is as defined herein before,
  • the preparations may be carried out in aqueous, alcoholic or chlorohalogenated media at ambient or higher temperatures.
  • the group IB plating species preferably comprises copper, the group IMA plating species comprises gallium and indium and the group VIA plating species comprises selenium and sulfur.
  • the metal plating composition comprises copper as the group IB plating species, gallium and/or indium as the group IMA plating species and selenium and/or sulfur as the VIA plating species.
  • the following species are particularly preferred plating species for use in the metal plating composition according to the present invention:
  • the copper plating species are copper sulphate, copper sulfamates or copper methanesulfamates and the indium plating species are indium sulfamates or indium methansulfamates.
  • the selenium plating species are comprised of selenous acid.
  • the complexing agents are contained in an amount of 0.001 to 2 mol/l, preferably 0.005 to 1 mol/l and most preferred 0.02 to 0.5 mol/l.
  • composition further comprises at least one wetting agent.
  • Uniclean® 399 is a mild alkaline, slightly foaming cleaner, which contains carbonate, silicates, phosphates, tensides and a biodegradable chelating agent. This bath is designed to remove mineral oils, polish and grind residues and pigment impurities for all metals.
  • the desired alloy such as a copper-indium- selenium alloy may be deposited on the substrate.
  • Pulse plating with two cathodic potentials (potentiostatic regime): -0.75 V for 0.9 s/-1.1 V for 0.1 s (potentials measured vs. Ag/AgCI electrode)
  • the alloys obtained in Examples 1 to 2 were subjected to a XRF surface scan.
  • the XRF (x-ray fluorescence) analysis is a non-destructive method.
  • the used equipment MocroXR 1200SV from Thermo-Fisher-Scientific, USA
  • the accelerating voltage is 47 keV. It is equipped with a polycapillary (0 3 mil; -76 ⁇ m).
  • the silicon drift detector (SDD) has a resolution of 163.3 eV (FWHM of Mn-Ka) and is Peltier cooled.
  • the samples are exposed to air, but due to a special geometric configuration and the evacuated beam and detector tubes it is possible to measure elements down to aluminium.
  • Fig. 1 shows the Cu/ln atomic ratio of the alloy obtained in Example 2 where no additive according to the present invention was contained in the metal plating bath. It is apparent from Fig. 1 that the Cu/ln atomic ratio varies with a standard deviation of nearly 16 %. Such a variation in the Cu/ln atomic ratio is much too high to produce a working solar cell on a 10 x 10 cm 2 substrate size (centered cut off a 15 x 15 cm 2 substrate - avoiding influences due to the inhomogeneities directly at the electrical contact).
  • Fig. 5 shows the Cu/ln ratio of the alloys obtained using the metal plating bath according to Example 1 and Example 2 as a result of varying rotating frequencies of the rotating disc electrode used.
  • the square root of the rotating frequency ( ⁇ ) is a measure for the hydrodynamic conditions within a galvanic bath.
  • Fig. 5 confirms that the Cu/ln ratio does not depend on the hydrodynamic conditions when a plating bath is used which comprises the additive ac- cording to the present invention (Example 1 ).
  • the Cu/ln ratio depends on the rotating frequency and thus on the hydrodynamic conditions that are present in the plating bath.
  • Fig. 5 also shows that it is possible to vary the Cu/ln ratio obtained in Example 1 (comprising the additive of the present invention) by varying the pH of the plating bath.
  • a lower pH corresponds to a lower Cu/ln ratio and a higher pH corresponds to a higher Cu/ln ratio, respectively.
  • Figs. 6a and 6b show the variation of a) the local electrochemical potential and b) the local current densities as a result of the external applied total current density. These values are measured directly on the Mo-coated float glass substrate at different distances to the electrical contact. The curves shown in Figs.
  • Figs. 7a and 7b show the stoichiometry (Cu/ln ratio) of electrodeposited CISe precursor in dependence of a) applied potential and b) applied current density on Mo coated float glass as well as the electrolyte behaviour according to the invention (Example 1 ).
  • the horizontal sections in both curves show the operating range wherein a constant alloy composition can be achieved using the additives according to the present invention.
  • the inventive additive according to formula IV was used for deposition of copper in a low acid copper bath with the following composition:

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Electrochemistry (AREA)
  • Computer Hardware Design (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Power Engineering (AREA)
  • Electromagnetism (AREA)
  • Physics & Mathematics (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Physics & Mathematics (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Inorganic Chemistry (AREA)
  • Electroplating And Plating Baths Therefor (AREA)
  • Photovoltaic Devices (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
PCT/EP2009/003885 2008-05-30 2009-05-29 Electroplating additive for the deposition of metal, a binary, ternary, quaternary or pentanary alloy of elements of group 11 (ib)-group 13 (iiia) -group 16 (via) WO2009144036A1 (en)

Priority Applications (3)

Application Number Priority Date Filing Date Title
US12/995,078 US8828278B2 (en) 2008-05-30 2009-05-29 Electroplating additive for the deposition of metal, a binary, ternary, quaternary or pentanary alloy of elements of group 11 (IB)—group 13 (IIIA)—Group 16 (VIA)
JP2011510899A JP5286410B2 (ja) 2008-05-30 2009-05-29 １１（ｉｂ）族−１３（ｉｉｉａ）族−１６（ｖｉａ）族の元素の、２成分、３成分、４成分もしくは５成分系合金を推積させるための電気メッキ用添加剤
CN2009801194459A CN102047438B (zh) 2008-05-30 2009-05-29 用于11(ib)族-13(iiia)族-16(via)族元素的金属、二元、三元、四元或五元合金沉积的电镀添加剂

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
EP08009979.9 2008-05-30
EP08009979.9A EP2128903B1 (en) 2008-05-30 2008-05-30 Electroplating additive for the deposition of a metal, a binary, ternary, quaternary or pentanary alloy of elements of group 11 (IB)-group 13 (IIIA)-group 16 (VIA)

Publications (1)

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WO2009144036A1 true WO2009144036A1 (en) 2009-12-03

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Country Status (6)

Country Link
US (1) US8828278B2 (ja)
EP (1) EP2128903B1 (ja)
JP (1) JP5286410B2 (ja)
CN (1) CN102047438B (ja)
ES (1) ES2624637T3 (ja)
WO (1) WO2009144036A1 (ja)

Cited By (1)

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JP2013536986A (ja) * 2010-09-02 2013-09-26 インターナショナル・ビジネス・マシーンズ・コーポレーション ガリウムおよびガリウム合金膜の電着方法ならびに関連する光起電構造

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US20110108115A1 (en) * 2009-11-11 2011-05-12 International Business Machines Corporation Forming a Photovoltaic Device
US8304272B2 (en) 2010-07-02 2012-11-06 International Business Machines Corporation Germanium photodetector
US8545689B2 (en) 2010-09-02 2013-10-01 International Business Machines Corporation Gallium electrodeposition processes and chemistries
US8840770B2 (en) * 2010-09-09 2014-09-23 International Business Machines Corporation Method and chemistry for selenium electrodeposition
JP5552042B2 (ja) 2010-12-27 2014-07-16 インターナショナル・ビジネス・マシーンズ・コーポレーション プログラム解析の方法、システムおよびプログラム
US20130327652A1 (en) * 2012-06-07 2013-12-12 International Business Machines Corporation Plating baths and methods for electroplating selenium and selenium alloys
US9495989B2 (en) 2013-02-06 2016-11-15 International Business Machines Corporation Laminating magnetic cores for on-chip magnetic devices
CN103924269B (zh) * 2013-12-26 2016-04-13 苏州昕皓新材料科技有限公司 一种非染料系整平剂的应用
CN103924268B (zh) * 2013-12-26 2016-04-13 苏州昕皓新材料科技有限公司 一种酸铜整平剂的应用
CN105696035A (zh) * 2016-04-18 2016-06-22 程敏敏 一种高性能填孔镀铜溶液

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Publication number Priority date Publication date Assignee Title
JP2013536986A (ja) * 2010-09-02 2013-09-26 インターナショナル・ビジネス・マシーンズ・コーポレーション ガリウムおよびガリウム合金膜の電着方法ならびに関連する光起電構造
US9401443B2 (en) 2010-09-02 2016-07-26 International Business Machines Corporation Electrodeposition methods of gallium and gallium alloy films and related photovoltaic structures

Also Published As

Publication number Publication date
US20110094583A1 (en) 2011-04-28
ES2624637T3 (es) 2017-07-17
JP2011524945A (ja) 2011-09-08
US8828278B2 (en) 2014-09-09
EP2128903B1 (en) 2017-02-22
CN102047438A (zh) 2011-05-04
EP2128903A1 (en) 2009-12-02
CN102047438B (zh) 2013-10-09
JP5286410B2 (ja) 2013-09-11

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